CN107955413A - A kind of preparation method for applying the conductive filler on electrically conductive ink - Google Patents
A kind of preparation method for applying the conductive filler on electrically conductive ink Download PDFInfo
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- CN107955413A CN107955413A CN201711297646.0A CN201711297646A CN107955413A CN 107955413 A CN107955413 A CN 107955413A CN 201711297646 A CN201711297646 A CN 201711297646A CN 107955413 A CN107955413 A CN 107955413A
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- Prior art keywords
- ink
- preparation
- conductive filler
- minutes
- electrically conductive
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
Abstract
The present invention relates to ink-printing techniques field, disclose a kind of preparation method for applying the conductive filler on electrically conductive ink, the conductive filler being prepared applies the electric conductivity on electrically conductive ink to stablize, it can almost mix with any solvent, good dispersion, preparation process is simple, it during ink uses and stores is not in reunion or precipitation that silver, which is coated with silicon-carbide particle as conducting particles, because its own not easily passs through Van der Waals force reunion and precipitate, the electric conductivity of ink will not decline over time, storge quality is high, it is high with dispersant fitness, it will not hinder the contact between particle, improve the electric conductivity of ink again at the same time, wetting of the matrix resin to conductive filler granule surface is high, conductive particle dispersiveness and storage stability in ink is very excellent.
Description
Technical field
The invention belongs to ink-printing techniques field, and in particular to a kind of system for applying the conductive filler on electrically conductive ink
Preparation Method.
Background technology
Ink is the important materials for packaging material printing, it is shown pattern, word on stock by printing
Ink includes main component and auxiliary element, they equably mix and form a kind of sticky colloidal fluid through repeat-rolling.
Ink is constantly riseing as necessary raw material during color printing, demand, and China's ink industry production in 2010, which has reached, goes through
History highest level,《Chinese ink industry production and marketing demand is looked forward to the prospect with investment forecasting analysis report》Statistics, national ink gross annual output amount
58.99 ten thousand tons altogether, exceed Germany first, Japan occupies the second in the world.Come according to about 4,100,000 tons of world's ink annual output then
Calculate, Chinese Printing ink producing scale accounts for the 14% of the whole world.
The preparation method of the conductive filler on electrically conductive ink is applied, with conductive material (gold, silver, the copper and carbon) company of being dispersed in
Manufactured paste-like ink, is commonly called as paste ink in ramming material.With conduction property to a certain degree, printing conductiving point or conduction can be used as
Circuit is used.Gold system conductive ink, silver system conductive ink, copper system conductive ink, carbon series conductive ink etc. have reached practical, for printing electricity
The materials such as road, electrode, plating bottom, keyboard contact, printed resistor.
Now with the development of 3D printing technique, the development of electrically conductive ink has huge development space, and wherein conduction is filled out
Material is the nucleus of electrically conductive ink, it is the function phase for determining ink electric conductivity.
The content of the invention
The purpose of the present invention is for it is existing the problem of, there is provided a kind of system for applying the conductive filler on electrically conductive ink
Preparation Method, the conductive filler for obtaining excellent performance are applied on electrically conductive ink.
The present invention is achieved by the following technical solutions：
A kind of preparation method for applying the conductive filler on electrically conductive ink, preparation method comprise the following steps：
（1）Take 2.8-3.0 moles of silicon carbide powder to be put into beaker, 150-200 milliliters of deionized water is added, in 350-
Stir under 400 revs/min 20-30 minutes, be then ultrasonically treated 15-20 minutes, continue stirring 50-60 minutes, then in 1500-
1800 revs/min centrifugal treating 3-5 minutes lower, outwells supernatant liquor, and the precipitation of lower floor is taken out and is placed in baking oven, in 60-70
When dry 6-8 is small at DEG C, the carborundum powder that is pre-processed；
（2）According to mass ratio it is 1 by pretreated carborundum powder and the concentrated sulfuric acid：The ratio mixing of 4-6, under 0-5 DEG C of water-bath
Stirring 30-40 minute, is then added three times the potassium permanganate that mass fraction is 8-10%, stirring is lower react 2-3 it is small when, then by
Drop ground add 15-18% volume fractions hydrogen peroxide, reaction 1-2 it is small when after obtain oxidation suspension, at 1500-1800 revs/min
Lower centrifugal treating 3-5 minutes, outwells supernatant liquor, and the precipitation of lower floor is used deionized water centrifuge washing 2-3 times；
（3）Wash and the silver nitrate that mass fraction is 6-7% and the poly- second that mass fraction is 45-55% are added in backward oxide precipitate
Alkene pyrrolidone, stirs 20-30 minutes under 300-350 revs/min, mix and blend thing is added to and is heated to reflux in device,
Open condensed water and open mechanical agitation, be warming up to 90-100 DEG C, the concentration that 1.2-1.3 times of volume is added dropwise is 1.0-1.2
G/l sodium borohydride solution, after adding under 100-110 DEG C of oil bath heating react 3.5-4.5 it is small when, after having reacted, will produce
Thing is washed with deionized 3-5 times and dries in an oven to constant weight.
Further described as to such scheme, step（1）Described in silicon carbide powder particle size at 1-10 microns
Between.
Further described as to such scheme, step（2）Described in the concentration of the concentrated sulfuric acid be 96-98%.
Further described as to such scheme, step（3）Described in sodium borohydride solution rate of addition for 3-4 milli
Liter/min.
Further described as to such scheme, addition mass percent of the conductive filler in ink is 4.5-
5.5%。
The present invention has the following advantages compared with prior art：In order to solve existing conductive filler, application performance is not on electrically conductive ink
The problem of good, the present invention provides a kind of preparation method for applying the conductive filler on electrically conductive ink, the conduction being prepared
Applying filler electric conductivity on electrically conductive ink is stablized, and can almost mix with any solvent, good dispersion, preparation process letter
Single, silver is coated with silicon-carbide particle as conducting particles and during ink uses and stores is not in reunion or precipitation, because
Its own not easily passs through Van der Waals force and reunites and precipitate, and the electric conductivity of ink will not decline over time, storage
Performance is high, high with dispersant fitness, will not hinder the contact between particle, while improve the electric conductivity of ink, base again
Wetting of the body resin to conductive filler granule surface is high, and conductive particle dispersiveness and storage stability in ink is very excellent,
Conductivity reaches
6.5·106-7.0·106S/m。
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method for applying the conductive filler on electrically conductive ink, preparation method comprise the following steps：
（1）Take 2.8 moles of silicon carbide powders to be put into beaker, add 150 milliliters of deionized water, stirred under 350 revs/min
Mix 20 minutes, be then ultrasonically treated 15 minutes, continue stirring 50 minutes, then in 1500 revs/min of lower centrifugal treatings 3 minutes,
Outwell supernatant liquor, the precipitation of lower floor taken out and is placed in baking oven, at 60 DEG C it is dry 6 it is small when, the carborundum that is pre-processed
Powder；
（2）According to mass ratio it is 1 by pretreated carborundum powder and the concentrated sulfuric acid：4 ratio mixing, is stirred under 0 DEG C of water-bath
30 minutes, the potassium permanganate that mass fraction is 8% is then added three times, when reaction 2 is small under stirring, is then dropwisely added 15%
The hydrogen peroxide of volume fraction, when reaction 1 is small after obtain oxidation suspension, in 1500 revs/min of lower centrifugal treatings 3 minutes, outwell
Supernatant liquor, deionized water centrifuge washing is used 2 times by the precipitation of lower floor；
（3）Wash and the silver nitrate that mass fraction is 6% and the polyethylene pyrrole that mass fraction is 45% are added in backward oxide precipitate
Pyrrolidone, stirs 20 minutes under 300 revs/min, mix and blend thing is added to and is heated to reflux in device, opens condensed water simultaneously
Mechanical agitation is opened, is warming up to 90 DEG C, the concentration that 1.2 times of volumes are added dropwise is 1.0 g/l of sodium borohydride solution, is added
When reaction 3.5 is small under 100 DEG C of oil bath heatings afterwards, after having reacted, product is washed with deionized 3 times and is dried in an oven extremely
Constant weight.
Further described as to such scheme, step（1）Described in silicon carbide powder particle size at 1-10 microns
Between.
Further described as to such scheme, step（2）Described in the concentrated sulfuric acid concentration be 96%.
Further described as to such scheme, step（3）Described in sodium borohydride solution rate of addition for 3 milli
Liter/min.
Further described as to such scheme, addition mass percent of the conductive filler in ink is
4.5%。
Embodiment 2
A kind of preparation method for applying the conductive filler on electrically conductive ink, preparation method comprise the following steps：
（1）Take 2.9 moles of silicon carbide powders to be put into beaker, add 180 milliliters of deionized water, stirred under 380 revs/min
Mix 25 minutes, be then ultrasonically treated 18 minutes, continue stirring 55 minutes, then in 1600 revs/min of lower centrifugal treatings 4 minutes,
Outwell supernatant liquor, the precipitation of lower floor taken out and is placed in baking oven, at 65 DEG C it is dry 7 it is small when, the carborundum that is pre-processed
Powder；
（2）According to mass ratio it is 1 by pretreated carborundum powder and the concentrated sulfuric acid：5 ratio mixing, is stirred under 2 DEG C of water-baths
35 minutes, the potassium permanganate that mass fraction is 9% is then added three times, when reaction 2.5 is small under stirring, is then dropwisely added
The hydrogen peroxide of 16% volume fraction, when reaction 1.5 is small after obtain oxidation suspension, in 1600 revs/min of lower centrifugal treatings 4 minutes,
Supernatant liquor is outwelled, the precipitation of lower floor is used into deionized water centrifuge washing 2 times；
（3）Wash and the silver nitrate that mass fraction is 6.5% and the polyethylene that mass fraction is 50% are added in backward oxide precipitate
Pyrrolidones, stirs 25 minutes under 320 revs/min, mix and blend thing is added to and is heated to reflux in device, opens condensed water
And mechanical agitation is opened, 95 DEG C are warming up to, the concentration that 1.25 times of volumes are added dropwise is 1.1 g/l of sodium borohydride solution, is added
When reaction 4.0 is small under 105 DEG C of oil bath heatings after complete, after having reacted, product is washed with deionized 4 times and is dried in an oven
To constant weight.
Further described as to such scheme, step（1）Described in silicon carbide powder particle size at 1-10 microns
Between.
Further described as to such scheme, step（2）Described in the concentrated sulfuric acid concentration be 97%.
Further described as to such scheme, step（3）Described in sodium borohydride solution rate of addition for 3.5 milli
Liter/min.
Further described as to such scheme, addition mass percent of the conductive filler in ink is
5.0%。
Embodiment 3
A kind of preparation method for applying the conductive filler on electrically conductive ink, preparation method comprise the following steps：
（1）Take 3.0 moles of silicon carbide powders to be put into beaker, add 200 milliliters of deionized water, stirred under 400 revs/min
Mix 30 minutes, then in 1800 revs/min of lower centrifugal treatings 5 minutes, outwell supernatant liquor, the precipitation of lower floor is taken out and is placed in baking
In case, at 70 DEG C it is dry 8 it is small when, the carborundum powder that is pre-processed；
（2）According to mass ratio it is 1 by pretreated carborundum powder and the concentrated sulfuric acid：6 ratio mixing, is stirred under 5 DEG C of water-baths
40 minutes, the potassium permanganate that mass fraction is 10% is then added three times, when reaction 3 is small under stirring, is then dropwisely added 18%
The hydrogen peroxide of volume fraction, when reaction 2 is small after obtain oxidation suspension, in 1800 revs/min of lower centrifugal treatings 5 minutes, outwell
Supernatant liquor, deionized water centrifuge washing is used 3 times by the precipitation of lower floor；
（3）Wash and the silver nitrate that mass fraction is 7% and the polyethylene that mass fraction is 45-55% are added in backward oxide precipitate
Pyrrolidones, stirs 30 minutes under 350 revs/min, mix and blend thing is added to and is heated to reflux in device, opens condensed water
And mechanical agitation is opened, 100 DEG C are warming up to, the concentration that 1.3 times of volumes are added dropwise is 1.2 g/l of sodium borohydride solution, is added
When reaction 4.5 is small under 110 DEG C of oil bath heatings after complete, after having reacted, product is washed with deionized 5 times and is dried in an oven
To constant weight.
Further described as to such scheme, step（1）Described in silicon carbide powder particle size at 1-10 microns
Between.
Further described as to such scheme, step（2）Described in the concentrated sulfuric acid concentration be 98%.
Further described as to such scheme, step（3）Described in sodium borohydride solution rate of addition for 4 milli
Liter/min.
Further described as to such scheme, addition mass percent of the conductive filler in ink is
5.5%。
Claims (5)
1. a kind of preparation method for applying the conductive filler on electrically conductive ink, it is characterised in that preparation method includes following step
Suddenly：
（1）Take 2.8-3.0 moles of silicon carbide powder to be put into beaker, 150-200 milliliters of deionized water is added, in 350-
Stir under 400 revs/min 20-30 minutes, be then ultrasonically treated 15-20 minutes, continue stirring 50-60 minutes, then in 1500-
1800 revs/min centrifugal treating 3-5 minutes lower, outwells supernatant liquor, and the precipitation of lower floor is taken out and is placed in baking oven, in 60-70
When dry 6-8 is small at DEG C, the carborundum powder that is pre-processed；
（2）According to mass ratio it is 1 by pretreated carborundum powder and the concentrated sulfuric acid：The ratio mixing of 4-6, under 0-5 DEG C of water-bath
Stirring 30-40 minute, is then added three times the potassium permanganate that mass fraction is 8-10%, stirring is lower react 2-3 it is small when, then by
Drop ground add 15-18% volume fractions hydrogen peroxide, reaction 1-2 it is small when after obtain oxidation suspension, at 1500-1800 revs/min
Lower centrifugal treating 3-5 minutes, outwells supernatant liquor, and the precipitation of lower floor is used deionized water centrifuge washing 2-3 times；
（3）Wash and the silver nitrate that mass fraction is 6-7% and the poly- second that mass fraction is 45-55% are added in backward oxide precipitate
Alkene pyrrolidone, stirs 20-30 minutes under 300-350 revs/min, mix and blend thing is added to and is heated to reflux in device,
Open condensed water and open mechanical agitation, be warming up to 90-100 DEG C, the concentration that 1.2-1.3 times of volume is added dropwise is 1.0-1.2
G/l sodium borohydride solution, after adding under 100-110 DEG C of oil bath heating react 3.5-4.5 it is small when, after having reacted, will produce
Thing is washed with deionized 3-5 times and dries in an oven to constant weight.
A kind of 2. preparation method for applying the conductive filler on electrically conductive ink as claimed in claim 1, it is characterised in that step
（1）Described in silicon carbide powder particle size between 1-10 microns.
A kind of 3. preparation method for applying the conductive filler on electrically conductive ink as claimed in claim 1, it is characterised in that step
（2）Described in the concentration of the concentrated sulfuric acid be 96-98%.
A kind of 4. preparation method for applying the conductive filler on electrically conductive ink as claimed in claim 1, it is characterised in that step
（3）Described in the rate of addition of sodium borohydride solution be 3-4 ml/mins.
5. a kind of preparation method for applying the conductive filler on electrically conductive ink as claimed in claim 1, it is characterised in that described
Addition mass percent of the conductive filler in ink is 4.5-5.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711297646.0A CN107955413A (en) | 2017-12-08 | 2017-12-08 | A kind of preparation method for applying the conductive filler on electrically conductive ink |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711297646.0A CN107955413A (en) | 2017-12-08 | 2017-12-08 | A kind of preparation method for applying the conductive filler on electrically conductive ink |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109887638A (en) * | 2019-01-14 | 2019-06-14 | 上海大学 | The multi-dimension nano silver paste and preparation method thereof that nano-Ag particles are mixed with silver-plated silicon-carbide particle |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1636938A (en) * | 2004-11-26 | 2005-07-13 | 中国科学院长春应用化学研究所 | Silicon carbide surface modifying method |
| CN102400121A (en) * | 2011-11-05 | 2012-04-04 | 上海上大瑞沪微系统集成技术有限公司 | Preparation process of nano ceramic particles for reinforcing composite lead-free solder |
| WO2015181706A1 (en) * | 2014-05-27 | 2015-12-03 | Auckland Uniservices Limited | Plating or coating method for producing metal-ceramic coating on a substrate |
-
2017
- 2017-12-08 CN CN201711297646.0A patent/CN107955413A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1636938A (en) * | 2004-11-26 | 2005-07-13 | 中国科学院长春应用化学研究所 | Silicon carbide surface modifying method |
| CN102400121A (en) * | 2011-11-05 | 2012-04-04 | 上海上大瑞沪微系统集成技术有限公司 | Preparation process of nano ceramic particles for reinforcing composite lead-free solder |
| WO2015181706A1 (en) * | 2014-05-27 | 2015-12-03 | Auckland Uniservices Limited | Plating or coating method for producing metal-ceramic coating on a substrate |
Non-Patent Citations (2)
| Title |
|---|
| 张允诚等: "《电镀手册》", 31 January 2017, 北京:国防工业出版社 * |
| 李文良等: "化学镀银在复合粉体中的应用及研究进展", 《电镀与精饰》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109887638A (en) * | 2019-01-14 | 2019-06-14 | 上海大学 | The multi-dimension nano silver paste and preparation method thereof that nano-Ag particles are mixed with silver-plated silicon-carbide particle |
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Application publication date: 20180424 |